Synthesis method of tetra(para-tolyl)stibonium benzenesulfonate from tetra(para-tolyl)stibonium chloride and benzenesulphonic acid

The interaction of tetra(para-tolyl)stibonium chloride p-Tol4SbCl (1) with benzenesulfonic acid was used to synthesize tetra(para-tolyl)stibonium benzenesulfonate p-Tol4SbOSO2Ph (2). The structure of compounds 1, 2 was established by X-ray diffraction analysis (XRD). According to XRD data, tetra(para-tolyl)stibonium chloride p-Tol4SbCl (1) [C28H28ClSb, M = 521,70; monoclinic syngony, sp. gr. P21/n; cell parameters: a = 9.786(3) Å, b = 23.168(8) Å, c = 12.026(5) Å; a = 90.00°, β = 113.689(16)°, g = 90.00°, V = 2496.6(16) Å3, Z = 4; r(calc.) = 1.388 g/cm3; m = 1.224 mm-1; F(000) = 1056.0; region 2q collection: 6.44-56.72°; -13 ≤ h ≤ 13, -30 ≤ k ≤ 30, -15 ≤ l ≤ 15; total reflections 59454; independent reflections 6189 (Rint = 0.0394); GOOF = 1.055; R-factor 2.72%] has a molecular structure with a distorted trigonal-bipyramidal coordination of the antimony atom (the CSbC angles vary within 96.12(8)-124.83(8)°, the CSbCl axial angle is 174.91(6)°, the Sb-C and Sb-Cl distances are 2.107(2)-2.170(2) and 2.7230(13) Å). Tetra(para-tolyl)stibonium benzenesulfonate p-Tol4SbOSO2Ph (2) [C34H33O3SSb, M = 643,1; rhombic system, sp. gr. Pbca; cell parameters: a = 9.923(8) Å, b = 18.923(16) Å, c = 32.72(3) Å; a = 90.00°, β = 90.00°, g = 90.00°, V = 6146(9) Å3, Z = 8; r(calc.) = 1.391 g/cm3; m = 0.997 mm-1; F(000) = 2624.0; region collection for 2q: 5.954-56.644°; -8 ≤ h ≤ 12, -25 ≤ k ≤ 25, -43 ≤ l ≤ 43; total reflections 73682; independent reflections 7553 (Rint = 0.0589); GOOF = 1.076; R-factor 4.93%, the CSbC angles vary within 97.72(14)-118.77(15)°, the CSbO axial angle is 176.44(13)°, the Sb-C and Sb-O distances are 2.105(4)-2.150(4) and 2.409(3) Å] has similar structure. Complete tables of atomic coordinates, bond lengths, and bond angles for compounds 1 and 2 have been deposited with the Cambridge Crystallographic Data Centre (CCDC 2167562 and 2126493) and are available, free of charge, at deposit@ccdc.cam.ac.uk and http://www.ccdc.cam.ac.uk.